CN104889411A - Machining medium for preparing graphene and method for preparing graphene composite material and graphene - Google Patents
Machining medium for preparing graphene and method for preparing graphene composite material and graphene Download PDFInfo
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- CN104889411A CN104889411A CN201510252239.2A CN201510252239A CN104889411A CN 104889411 A CN104889411 A CN 104889411A CN 201510252239 A CN201510252239 A CN 201510252239A CN 104889411 A CN104889411 A CN 104889411A
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Abstract
The invention discloses a machining medium for preparing graphene and a method for preparing a graphene composite material and the graphene. The machining medium is a metal material, and the metal material and graphite serving as a raw material are mixed when the metal material is used for machining to obtain the graphene or the metal matrix graphene composite material. The graphene composite material and the graphene can be obtained as needed by the aid of the medium and a proper machining mode, the machining medium is better in yield rate and higher in product quality, any types of graphite directly serves as the raw material, and pretreatment such as oxidation and expansion at an early stage can be omitted. By the aid of pure physical effects, the graphene is complete in thin layer structure, pure in product and free of any other organic groups such as oxygen and nitrogen or inorganic impurities except for carbon, metal is easily removed and can be recovered by methods such as hot melting or electrochemistry, the machining medium is repeatedly used, safe, environmentally friendly, recyclable and easy in extensive industrialization production, and waste discharge is avoided.
Description
Technical field
The present invention relates to a kind of processing technology of Graphene, particularly a kind of machining medium for the preparation of Graphene, prepare the method for graphene composite material and Graphene.
Background technology
Graphene is the nano material with excellent transparent, heat conductivility and lower resistivity, is expected to can be used to develop thinner, conduction speed electronic component of new generation or transistor faster; Also can be used to manufacture transparent touch screen, tabula rasa or even solar cell.
In prior art, the preparation method of Graphene mainly:
Chemical vapour deposition (CVD), the quality of graphene of acquisition is good, area is large; But cost is high, equipment is complicated, technological requirement is high, and quantum of output is extremely low, is not suitable for suitability for industrialized production;
Oxidation-reduction method, initial oxidation, needs secondary reduction, and product structure introduces defect, and chemical contamination is serious, is also not suitable for suitability for industrialized production;
Solvent is peeled off, and product Graphene prototype structure retains complete; The solvability of graphite is limited, and productive rate is low;
Ball-milling method: by direct high-energy ball milling or add medium (dry ice, oxide etc.) Graphite, obtains Graphene; Direct high-energy ball milling ball-milling method productive rate is lower, and energy consumption is higher; Add in medium mechanical milling process, the particle after fragmentation and graphite contact mostly are point cantact, reduce mechanical energy on the one hand and are shifted by the transmission of these particles to graphite; Be easy on the other hand cause the fracture of graphite broken, instead of splitting, be unfavorable for retaining large stretch of graphite flake layer, therefore the productive rate of thin layer graphite and Graphene is not high.
Particularly, Graphene is utilized to form required composite, such as to obtain the Metal Substrate graphene composite conductive material with higher-strength, then need comparatively complicated technical process, or the preparation method forming composite and Graphene itself there is no and contacts directly, and needs multiple working procedure, cause the complexity of equipment, technique, improve process costs.
Therefore, need to improve the preparation method of Graphene, adopt suitable processing mode, composite and Graphene itself can be associated, there is good output capacity and higher product quality, be applicable to suitability for industrialized production, reduce costs.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of machining medium for the preparation of Graphene, prepare the method for graphene composite material and Graphene, this medium is utilized to adopt suitable machining mode, graphene composite material and Graphene can be obtained as required, there is good output capacity and higher product quality, be applicable to suitability for industrialized production, reduce costs.
A kind of machining medium for the preparation of Graphene of the present invention, described medium is metal, and described metal is used for mixing with raw graphite when machining obtains Graphene or Metal Substrate graphene composite material.
Further, described metal has required plasticity, elongation at break >2%;
Further, described metal is metal powder material;
Further, the fineness of described metal powder material is suitable with the fineness of the raw graphite for obtaining Graphene;
Further, the metal of described metal powder material is a kind of, several mixture in gold, silver, copper, aluminium, magnesium, iron, zinc, sodium, calcium, lithium, titanium, nickel, tin, lead or with this metal alloy.
The invention also discloses a kind of method utilizing described medium to prepare graphene composite material, comprise the following steps:
A. metal material and raw graphite are thrown in in machining equipment;
B. the machining mode with the effect of rolling is adopted to carry out machining;
C. discharging, namely obtains Metal Substrate graphene composite material.
Further, in step a, described machining equipment is closed and is adopted inert gas shielding or vacuum;
Further, in step b, described machining adopts ball milling, grinds, mills or sand milling, if employing ball milling, ball material volume ratio is 3-100:1, and described metal material is metal powder material, and raw material Raw graphite and metal powder material volume ratio are 1:0.2-30;
Further, in described ball milling, ball grinder filling rate is not more than 50%; Ball-milling Time: 1h-100h.
The invention also discloses and a kind ofly utilize described medium to prepare Graphene method, adopt the mode of hot melt or acid dissolve to remove on the metal of prepared Graphene/metallic composite and namely obtain Graphene.
Beneficial effect of the present invention: the machining medium for the preparation of Graphene of the present invention, prepare the method for graphene composite material and Graphene, adopt the metal dust with suitable plastic as machining medium, in mechanical processing process, Graphene or graphite flake and sheet metal, through the machining of certain hour, under the External Force Acting that impact, shearing, friction etc. are comprehensive, the carbon-metal interface of metal-graphite group remains intact, and graphite carbon-coating model ylid bloom action can be removed by mechanical energy, graphite flake layer is stripped as Graphene individual layer or lamella; In above-mentioned technical process, adopt the less soft metal of hardness can also reduce the fragmentation of graphite, make larger thin layer graphite sheet and Graphene be able to part and retain; Can be formed directly in Metal Substrate graphene composite material as required, and obtain Graphene after (acid dissolve or hot melt) metal can be removed; Therefore, this medium is utilized to adopt suitable machining mode, graphene composite material and Graphene can be obtained as required, there is good output capacity and higher product quality, directly use any type graphite to be raw material, can without the need to doing the pretreatment such as early stage oxidation, expansion, adopt pure physical action, Graphene laminate structure is complete, products pure, except carbon, any other organic group or the inorganic impurity such as oxygen-free, nitrogen; Metal is easy to remove, and the method such as available hot melt or electrochemistry reclaims, and recycles, safety and environmental protection, no waste discharge, has recyclability, be easy to large-scale industrial production.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention will be further described.
Fig. 1 is Graphene and thin layer graphite product transmission electron microscope picture.
Detailed description of the invention
The machining medium for the preparation of Graphene of the present embodiment, described medium is metal, described metal is used for mixing with raw graphite when machining obtains Graphene or Metal Substrate graphene composite material, metal can be Powdered, can be less particle, strip etc., all goal of the invention can be realized, select according to different needs, generally select metal dust, have and be easy to mixed performance preferably; Carry out machining after metal powder material mixes with graphite, machining here comprises the Graphene mechanical processing technique of traditional handicraft, such as ball milling, roll.
In the present embodiment, described metal has required plasticity, elongation at break >2%; Need according to different the metal selecting different plasticity, generally softer metal can obtain large stretch of layer graphene or thin layer graphite.
In the present embodiment, described metal is metal powder material; Metal powder material has good Combination, and can form the corresponding relation of particle comparatively uniformly with raw graphite, adds and has better manufacturability man-hour.
In the present embodiment, the fineness of described metal powder material is suitable with the fineness of the raw graphite for obtaining Graphene; The metal dust of this fineness is beneficial to increases metal itself and the contact surface of graphite, is beneficial to the larger lamella of acquisition.
In the present embodiment, the metal of described metal powder material is a kind of, several mixture in gold, silver, copper, aluminium, magnesium, iron, zinc, sodium, calcium, lithium, titanium, nickel, tin, lead or with this metal alloy.
The invention also discloses a kind of method utilizing described medium to prepare graphene composite material, comprise the following steps:
A. metal material and raw graphite are thrown in in machining equipment;
B. the machining mode with the effect of rolling is adopted to carry out machining;
C. discharging, namely obtains Metal Substrate graphene composite material.
In the present embodiment, in step a, described machining equipment is closed and is adopted inert gas shielding or vacuum; Ensure that metal material is not oxidized in process, thus ensure final product quality.
In the present embodiment, in step b, described machining adopts ball milling, grinds, mills or sand milling.
In the present embodiment, in step b, described machining adopts ball milling, and ball material volume ratio is 3-100:1, preferred 9:2, and ball material volume ratio refers to the volume ratio of ball in ball grinder and raw material, and raw material is the mixture of metal powder material and graphite; Raw material Raw graphite and metal powder material volume ratio are 1:0.2-30, preferred 1:1; The ball milling batching reasonable coordination metal of above-mentioned parameter scope and the physical property of graphite itself, more can be adapted to the physical action between metal and graphite, be beneficial to and ensure low input and high yield.
In the present embodiment, in described ball milling, ball grinder filling rate is not more than 50%, i.e. (steel ball+raw material accounts for the percentage of the volume of ball grinder), and preferably 30%; Can vibratory milling be adopted in mechanical milling process, ball milling vibration frequency: 0-2000 week/min, preferably 1200 weeks/min; Ball-milling Time: 1h-100h, preferred about 6h; Ball milling parameter is determined according to the physical condition of metal and graphite itself, mutually coordinates mutual restriction with batching parameter, to obtain best product quality.
Method of the present invention, because metal or alloy is preferably easy to the metal or alloy of plastic deformation, abrading-ball impacts that metallic particles or powder can make it be out of shape, tear, refinement, fragmentation, the metal high energy surface of the raw new life of not stopping pregnancy; Quite or to be biggerly advisable, object is the contact surface increasing metal and graphite for the fineness of raw metal and graphite raw material;
In mechanical milling process, when the surge of abrading-ball forces metal to be pounded to graphite surface, metal is stressed upon graphite surface distortion, metallic atom and graphite surface atomic contacts area can be made to increase, it is one that metal and graphite are adhered mutually, namely metal is ground thin and is spread over graphite granule surface, or parcel graphite forms " metal-graphite granule ".
According to metal, there is higher surface energy (or surface tension), ball mill crushing goes out newborn metal surface and has powerful adsorption activity, metal surface atom pair graphite carbon-coating produces stronger absorption, adhesion interacts, when metallic graphite carbon contact faying face large to a certain extent time, metal-carbon layer interacts the model ylid bloom action (micromechanics is peeled off and proved that model ylid bloom action is more weak) be greater than between graphite carbon-coating.When " metal-graphite granule " is subject to abrading-ball impact again, the plane of disruption must be the most weak faying face---i.e. graphite layers faying face, graphite synusia is stripped to expand into and newborn exposes graphite surface, can be adhered with metal surface by abrading-ball collision again in this surface in mechanical milling process, form new " metal-graphite granule " again to peel off, graphite linings is thinned again.Through adhesion-stripping-adhesion-stripping process repeatedly, graphite is finally thinned to Graphene individual layer or thin layer.Meanwhile, in mechanical milling process, metal, constantly by impact grinding, produces fresh surface and is combined with thin layer graphite.
Therefore, through the ball milling of certain hour, under the External Force Acting that impact, shearing, friction etc. are comprehensive, the carbon-metal interface of metal-graphite group remains intact, and graphite carbon-coating model ylid bloom action can be removed by mechanical energy, graphite flake layer is stripped as Graphene individual layer or lamella.In addition, as the fragmentation adopting the less soft metal of hardness can also reduce graphite, make larger thin layer graphite sheet and Graphene be able to part and retain.
The invention also discloses and a kind ofly utilize described medium to prepare Graphene method, adopt the mode of hot melt or chemolysis to remove on the metal of prepared Metal Substrate graphene composite material and namely obtain Graphene; The acquisition of this graphene product is on the basis based on Metal Substrate graphene composite material, removes metal and obtains; Required material can be obtained by same technological process, cost-saving and ensure product quality; Metal removal method preferably utilizes chemolysis (generally comprise the mode of acid dissolve, alkali dissolving, do not repeat them here) and washing is dry, and technique is simple; For metal, after acid dissolve, carry out electrochemical deposition Footwall drift, and can again recycle; Also can heat fused separating metal, Footwall drift also can recycle again.
Under be classified as the specific embodiment of the preparation method of Graphene of the present invention and composite:
Embodiment one
The medium of the present embodiment prepares the method for graphene composite material, comprises the following steps:
A. metal powder material and raw graphite are thrown in in spheroidal graphite tank; Described spheroidal graphite potting is closed and is adopted inert gas shielding or vacuum; Described metal powder material is copper, and ball material volume ratio is 3:1, and raw material Raw graphite and copper powder volume ratio are 1:0.2, and in feeding intake, ball grinder filling rate is 10%, and the fineness of metal is 200 orders;
B. ball milling is carried out, in ball milling, ball milling friction, Ball-milling Time: 100h;
C. discharging, namely obtains copper-base graphite alkene composite.
Obtain Graphene and then need further following technique:
Adopt the mode of acid dissolve to remove the copper of the copper-base graphite alkene composite prepared by the present embodiment, namely obtain required Graphene to after remaining Graphene washing drying; Electrochemical deposition is carried out to the copper salt solution after pickling and reclaims copper, and can again recycle.
Embodiment two
The medium of the present embodiment prepares the method for graphene composite material, comprises the following steps:
A. metal powder material and raw graphite are thrown in in spheroidal graphite tank; Described spheroidal graphite potting is closed and is adopted inert gas shielding or vacuum; Described metal powder material is copper, and ball material volume ratio is 9:2, and raw material Raw graphite and copper powder volume ratio are 1:1, and in feeding intake, ball grinder filling rate is 30%, and the fineness of metal is 200 orders;
B. ball milling is carried out, in ball milling, ball milling vibration frequency: 1200 weeks/min, Ball-milling Time: 6h;
C. discharging, namely obtains copper-base graphite alkene composite.
Obtain Graphene and then need further following technique:
Adopt the mode of acid dissolve to remove the copper of the copper-base graphite alkene composite prepared by the present embodiment, namely obtain required Graphene to after remaining Graphene washing drying; Electrochemical deposition is carried out to the copper salt solution after pickling and reclaims copper, and can again recycle.
Embodiment three
The medium of the present embodiment prepares the method for graphene composite material, comprises the following steps:
A. metal powder material and raw graphite are thrown in in spheroidal graphite tank; Described spheroidal graphite potting is closed and is adopted inert gas shielding or vacuum; Described metal powder material is copper, and ball material volume ratio is 100:1, and raw material Raw graphite and copper powder volume ratio are 1:30, and in feeding intake, ball grinder filling rate is 50%, and the fineness of metal is 200 orders;
B. ball milling is carried out, in ball milling, ball milling vibration frequency: 2000 weeks/min, Ball-milling Time: 1h;
C. discharging, namely obtains copper-base graphite alkene composite.
Obtain Graphene and then need further following technique:
Adopt the mode of acid dissolve to remove the copper of the copper-base graphite alkene composite prepared by the present embodiment, namely obtain required Graphene to after remaining Graphene washing drying; Electrochemical deposition is carried out to the copper salt solution after pickling and reclaims copper, and can again recycle.
In above-described embodiment, metal powder material all adopts copper, in fact according to the character of theoretical foundation of the present invention and metal, adopts other metals with certain plasticity certainly also can realize goal of the invention; In above-described embodiment, the final graphene product obtained in embodiment two has preferably quality, has larger laminated structure, is most preferred embodiment; There is theoretical foundation of the present invention known, adopt softer metal and be equipped with rational ball milling parameter, the grapheme material of larger sheet needed for can obtaining, certainly, also can obtain larger metal-base composites.
Graphene metal-base composites of the present invention is ball milling product, in pulverulence, directly as battery electrode material, catalysis material, absorption gas storing material etc., also can carry out the following process such as cold and hot working and powder metallurgy process again, make block metal matrix composite.Certainly, ball milling product powder also can be used for, in various types of materials, not exemplifying at this as various additive or modifier.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (10)
1. for the preparation of a machining medium for Graphene, it is characterized in that: described medium is metal, described metal is used for mixing with raw graphite when machining obtains Graphene or Metal Substrate graphene composite material.
2. the machining medium for the preparation of Graphene according to claim 1, is characterized in that: described metal has required plasticity, elongation at break >2%.
3. according to the machining medium for the preparation of Graphene according to claim 1, it is characterized in that: described metal is metal powder material.
4. according to the machining medium for the preparation of Graphene according to claim 3, it is characterized in that: the fineness of described metal powder material is suitable with the fineness of the raw graphite for obtaining Graphene.
5. according to the machining medium for the preparation of Graphene according to claim 1, it is characterized in that: the metal of described metal powder material is a kind of, several mixture in gold, silver, copper, aluminium, magnesium, iron, zinc, sodium, calcium, lithium, titanium, nickel, tin, lead or with this metal alloy.
6. utilize the medium described in the arbitrary claim of claim 1 to 5 to prepare a method for graphene composite material, it is characterized in that: comprise the following steps:
A. metal and raw graphite are thrown in in machining equipment;
B. the machining mode with the effect of rolling is adopted to carry out machining;
C. discharging, namely obtains Metal Substrate graphene composite material.
7. according to the method preparing graphene composite material according to claim 6, it is characterized in that: in step a, described machining equipment is closed and is adopted inert gas shielding or vacuum.
8. according to the method preparing graphene composite material according to claim 7, it is characterized in that: in step b, described machining adopts ball milling, grinds, mills or sand milling, if employing ball milling, ball material volume ratio is 3-100:1, described metal adopts metal powder material, and raw material Raw graphite and metal powder material volume ratio are 1:0.2-30.
9. according to the method preparing graphene composite material according to claim 8, it is characterized in that: in described ball milling, ball grinder filling rate is not more than 50%; Ball-milling Time: 1h-100h.
10. utilize the medium described in the arbitrary claim of claim 1 to 5 to prepare a Graphene method, it is characterized in that: adopt the mode of hot melt or chemolysis to remove on the metal of the Graphene/metallic composite prepared by arbitrary for claim 6 to 9 claim and namely obtain Graphene.
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| CN111377438A (en) * | 2020-02-28 | 2020-07-07 | 清华大学 | Graphene and preparation method thereof |
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| CN104889411B (en) | 2020-06-12 |
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